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Method for separating and purifying chenodeoxycholic acid from goose bile

A technology of chenodeoxycholic acid and chenodeoxycholic acid, applied in the directions of steroids, organic chemistry, etc., can solve the problems of expanding chenodeoxycholic acid, etc., and achieve the effect of strong repeatability, high repeatability and improved effect.

Inactive Publication Date: 2013-10-23
四川新功生物科技集团有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to overcome the shortcomings of the existing extraction methods and expand the source of chenodeoxycholic acid, the present invention provides a method for separating and purifying chenodeoxycholic acid from goose bile, which simplifies the extraction while ensuring the yield and purity craft

Method used

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  • Method for separating and purifying chenodeoxycholic acid from goose bile
  • Method for separating and purifying chenodeoxycholic acid from goose bile
  • Method for separating and purifying chenodeoxycholic acid from goose bile

Examples

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Effect test

Embodiment 1

[0022] Preparation of crude chenodeoxycholic acid from goose bile

[0023] Take goose bile 200g (volume is 200mL) and put it in a beaker, add 6% sodium chloride solid by weight of bile, heat at 90°C for 10h for saponification, add calcium chloride solid of 8% by weight of bile after cooling to obtain precipitation, Collect the precipitate by centrifugation, dissolve the precipitate with distilled water 3 times the volume of the precipitate, stir for 50 minutes and collect the supernatant by centrifugation, adjust the pH to 3.0 with hydrochloric acid to obtain the precipitate, collect the precipitate by centrifugation, and dry the precipitate to obtain a khaki goose Oxycholic acid solid 5.32g.

Embodiment 2

[0025] Preparation of crude chenodeoxycholic acid from goose bile

[0026] Take goose bile 500g (volume is 500mL) and place in a beaker, add 8% sodium chloride solid by weight of bile, heat at 95°C for 15h for saponification, add 10% calcium chloride solid by weight of bile after cooling to obtain precipitation, Collect the precipitate by centrifugation, dissolve the precipitate with distilled water 3 times the volume of the precipitate, stir for 60 minutes and collect the supernatant by centrifugation, adjust the pH to 4.0 with hydrochloric acid to obtain the precipitate, collect the precipitate by centrifugal separation, and obtain the earthy yellow goose after the precipitate is dried Oxycholic acid solid 12.03g.

Embodiment 3

[0028] Purification of chenodeoxycholic acid

[0029] Take the crude chenodeoxycholic acid obtained in Example 1 or 2 and sodium hydroxide at a ratio of 1:1 and heat and dissolve in 25 times of water to form a chenodeoxycholic acid extract, and inject the extract into a 711-type macropore In the resin chromatography column, use 40% ethanol solution to elute until the effluent is colorless and transparent, then use 5% sodium hydroxide solution 4 times the weight of the extract to elute, collect the eluent, and use hydrochloric acid as the eluent Adjust the pH to 3.0, centrifuge to obtain chenodeoxycholic acid, dry, the yield of chenodeoxycholic acid is 1.32%, and the purity is 95% (see figure 1 ).

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Abstract

The invention provides a method for separating and purifying chenodeoxycholic acid from goose bile. Specifically, fresh goose bile is subjected to saponification, calcium precipitation, roughing and macro-porous resin purification to obtain a chenodeoxycholic acid pure product. The method has the advantages that (1) the raw material source of the chenodeoxycholic acid is expanded and the method for separating and purifying the chenodeoxycholic acid from the goose bile is provided, (2) compared with the conventional extraction process, ethyl acetate is not used any longer, the repeatability of experiments is increased, the environmental pollution is reduced and the recovery rate of the chenodeoxycholic acid is improved, and (3) compared with other macro-porous resin extraction methods, the operation is simplified and the recovery rate of the chenodeoxycholic acid is improved.

Description

technical field [0001] The invention relates to biochemical separation and purification, in particular to a method for separating and purifying chenodeoxycholic acid from goose bile. Background technique [0002] Chenodeoxycholic acid is a drug that dissolves stones. At present, it is mainly used in clinical treatment of gallstone disease and conversion into ursodeoxycholic acid to treat gallstones. Chenodeoxycholic acid is mainly extracted from animal bile. At present, most manufacturers extract chenodeoxycholic acid from chicken, duck bile and pig bile. There is still a lack of technology to extract chenodeoxycholic acid from goose bile. The development of goose farming and goose slaughtering and processing technology has greatly increased the source of goose bile, but the utilization rate of goose bile is still low at present, so goose bile can be used as a new source of chenodeoxycholic acid raw materials. [0003] The process of extracting chenodeoxycholic acid from c...

Claims

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Application Information

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IPC IPC(8): C07J9/00
Inventor 李全阳李冠霖
Owner 四川新功生物科技集团有限公司
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